Comparison of conventional liquid chromatography–tandem mass spectrometry versus microflow liquid chromatography–tandem mass spectrometry within the framework of full method validation for simultaneous quantification of 40 antidepressants and neuroleptics in whole blood

Steuer, Andrea E.; Poetzsch, Michael; Koenig, M. P.; Tingelhoff, Eva; Staeheli, Sandra N.; Roemmelt, Andreas T.; Kræmer, Thomas

doi:10.1016/j.chroma.2014.12.084

Cited by 35 publications

(35 citation statements)

References 36 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…SPE can be automated if higher throughput is desired. As already observed in earlier studies, MFLC still bears some drawbacks, the most severe being clogging of MFLC columns and ESI capillary . Occurrence of these problems appeared randomly and could not be correlated with a certain number of injections.…”

Section: Resultsmentioning

confidence: 69%

“…Therefore, the slight overlap was accepted in terms of throughput and robustness of the method. In a previous study on 40 antidepressants and neuroleptics, the MFLC system was prone to retention time shifts, especially with varying analyte concentrations. The same effect could not be observed in the current method on LSD and metabolites with stable retention times (+/‐ 0.02 min) observed over a time period of approximately four months and over the whole calibration range.…”

Section: Resultsmentioning

confidence: 99%

“…A previous study demonstrated similar performance characteristics in typical validation parameters for MFLC compared to conventional LC . However, despite its potential benefits, in the field of clinical and forensic toxicology such methods are currently scarce, possibly because these techniques are suspected to lack ruggedness …”

Section: Introductionmentioning

confidence: 85%

“…In general, scaling down flow rates to nano LC or MFLC systems led to certain benefits such as reduced solvent consumption, higher throughput through decreased run times, a higher ionization yield, and reduced ion suppression/enhancement effects . A previous study demonstrated similar performance characteristics in typical validation parameters for MFLC compared to conventional LC . However, despite its potential benefits, in the field of clinical and forensic toxicology such methods are currently scarce, possibly because these techniques are suspected to lack ruggedness …”

Section: Introductionmentioning

confidence: 99%

“…[28,29] A previous study demonstrated similar performance characteristics in typical validation parameters for MFLC compared to conventional LC. [30] However, despite its potential benefits, in the field of clinical and forensic toxicology such methods are currently scarce, possibly because these techniques are suspected to lack ruggedness. [28][29][30] The aim of the present study was the development and validation of a new, fast, and sensitive MFLC-MS/MS method for the validated quantification of LSD, iso-LSD, oxo-HO-LSD, and nor-LSD in plasma.…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

Development and validation of an ultra‐fast and sensitive microflow liquid chromatography‐tandem mass spectrometry (MFLC‐MS/MS) method for quantification of LSD and its metabolites in plasma and application to a controlled LSD administration study in humans

Steuer

Poetzsch

Stock

et al. 2016

Drug Testing and Analysis

Self Cite

View full text Add to dashboard Cite

Lysergic acid diethylamide (LSD) is a semi-synthetic hallucinogen that has gained popularity as a recreational drug and has been investigated as an adjunct to psychotherapy. Analysis of LSD represents a major challenge in forensic toxicology due to its instability, low drug concentrations, and short detection windows in biological samples. A new, fast, and sensitive microflow liquid chromatography (MFLC) tandem mass spectrometry method for the validated quantification of LSD, iso-LSD, 2-oxo 3-hydroxy-LSD (oxo-HO-LSD), and N-desmethyl-LSD (nor-LSD) was developed in plasma and applied to a controlled pharmacokinetic (PK) study in humans to test whether LSD metabolites would offer for longer detection windows. Five hundred microlitres of plasma were extracted by solid phase extraction. Analysis was performed on a Sciex Eksigent MFLC system coupled to a Sciex 5500 QTrap. The method was validated according to (inter)-national guidelines. MFLC allowed for separation of the mentioned analytes within 3 minutes and limits of quantification of 0.01 ng/mL. Validation criteria were fulfilled for all analytes. PK data could be calculated for LSD, iso-LSD, and oxo-HO-LSD in all participants. Additionally, hydroxy-LSD (HO-LSD) and HO-LSD glucuronide could be qualitatively detected and PK determined in 11 and 8 subjects, respectively. Nor-LSD was only sporadically detected. Elimination half-lives of iso-LSD (median 12 h) and LSD metabolites (median 9, 7.4, 12, and 11 h for oxo-HO-LSD, HO-LSD, HO-LSD-gluc, and nor-LSD, respectively) exceeded those of LSD (median 4.2 h). However, screening for metabolites to increase detection windows in plasma seems not to be constructive due to their very low concentrations. Copyright © 2016 John Wiley & Sons, Ltd.

show abstract

Section: Resultsmentioning

confidence: 69%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 85%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Development and validation of an ultra‐fast and sensitive microflow liquid chromatography‐tandem mass spectrometry (MFLC‐MS/MS) method for quantification of LSD and its metabolites in plasma and application to a controlled LSD administration study in humans

Steuer

Poetzsch

Stock

et al. 2016

Drug Testing and Analysis

Self Cite

View full text Add to dashboard Cite

show abstract

Fast simultaneous LC/MS/MS determination of 10 active compounds in human serum for therapeutic drug monitoring in psychiatric medication

Sistik

Urinovska

Brozmanová

et al. 2015

Biomedical Chromatography

View full text Add to dashboard Cite

A UPLC/MS/MS method with simple protein precipitation has been validated for the fast simultaneous analysis of agomelatine, asenapine, amisulpride, iloperidone, zotepine, melperone, ziprasidone, vilazodone, aripiprazole and its metabolite dehydro-aripiprazole in human serum. Alprenolol was applied as an internal standard. A BEH C18 (2.1 × 50 mm, 1.7 µm) column provided chromatographic separation of analytes using a binary mobile phase gradient (A, 2 mmol/L ammonium acetate, 0.1% formic acid in 5% acetonitrile, v/v/v; B, 2 mmol/L ammonium acetate, 0.1% formic acid in 95% acetonitrile, v/v/v). Mass spectrometric detection was performed in the positive electrospray ionization mode and ion suppression owing to matrix effects was evaluated. The validation criteria were determined: linearity, precision, accuracy, recovery, limit of detection, limit of quantification, reproducibility and matrix effect. The concentration range was as follows: 0.25-1000 ng/mL for agomelatine; 0.25-100 ng/mL for asenapine and iloperidone; 2.5-1000 ng/mL for amisulpride, aripiprazole, vilazodone and zotepine; 2.3-924.6 ng/mL for dehydroaripiprazole; 2.2-878.4 ng/mL for melperone; and 2.2-883.5 ng/mL for ziprasidone. Limits of quantitation below a therapeutic reference range were achieved for all analytes. Intra-run precision of 0.4-5.5 %, inter-run precision of 0.6-8.2% and overall recovery of 87.9-114.1% were obtained. The validated method was successfully implemented into routine practice for therapeutic drug monitoring in our hospital.

show abstract

Development of new extraction method based on liquid–liquid–liquid extraction followed by dispersive liquid–liquid microextraction for extraction of three tricyclic antidepressants in plasma samples

Farajzadeh

Abbaspour

2018

Biomedical Chromatography

View full text Add to dashboard Cite

In the present study, a new extraction method based on a three-phase system, liquid-liquid-liquid extraction, followed by dispersive liquid-liquid microextraction has been developed and validated for the extraction and preconcentration of three commonly prescribed tricyclic antidepressant drugs - amitriptyline, imipramine, and clomipramine - in human plasma prior to their analysis by gas chromatography-flame ionization detection. The three phases were an aqueous phase (plasma), acetonitrile and n-hexane. The extraction mechanism was based on the different affinities of components of the biological sample (lipids, fatty acids, pharmaceuticals, inorganic ions, etc.) toward each of the phases. This provided high selectivity toward the analytes since most interferences were transferred into n-hexane. In this procedure, a homogeneous solution of the aqueous phase (plasma) and acetonitrile (water-soluble extraction solvent) was broken by adding sodium sulfate (as a phase separating agent) and the analytes were extracted into the fine droplets of the formed acetonitrile. Next, acetonitrile phase was mixed with 1,2-dibromoethane (as a preconcentration solvent at microliter level) and then the microextraction procedure mentioned above was performed for further enrichment of the analytes. Under the optimum extraction conditions, limits of detection and lower limits of quantification for the analytes were obtained in the ranges of 0.001-0.003 and 0.003-0.010 μg mL , respectively. The obtained extraction recoveries were in the range of 79-98%. Intra- and inter-day precisions were < 7.5%. The validated method was successfully applied for determination of the selected drugs in human plasma samples obtained from the patients who received them.

show abstract

Comparison of conventional liquid chromatography–tandem mass spectrometry versus microflow liquid chromatography–tandem mass spectrometry within the framework of full method validation for simultaneous quantification of 40 antidepressants and neuroleptics in whole blood

Cited by 35 publications

References 36 publications

Development and validation of an ultra‐fast and sensitive microflow liquid chromatography‐tandem mass spectrometry (MFLC‐MS/MS) method for quantification of LSD and its metabolites in plasma and application to a controlled LSD administration study in humans

Development and validation of an ultra‐fast and sensitive microflow liquid chromatography‐tandem mass spectrometry (MFLC‐MS/MS) method for quantification of LSD and its metabolites in plasma and application to a controlled LSD administration study in humans

Fast simultaneous LC/MS/MS determination of 10 active compounds in human serum for therapeutic drug monitoring in psychiatric medication

Development of new extraction method based on liquid–liquid–liquid extraction followed by dispersive liquid–liquid microextraction for extraction of three tricyclic antidepressants in plasma samples

Contact Info

Product

Resources

About